JPH04194869A - Manufacture of electrostatic latent image developing toner - Google Patents
Manufacture of electrostatic latent image developing tonerInfo
- Publication number
- JPH04194869A JPH04194869A JP2320203A JP32020390A JPH04194869A JP H04194869 A JPH04194869 A JP H04194869A JP 2320203 A JP2320203 A JP 2320203A JP 32020390 A JP32020390 A JP 32020390A JP H04194869 A JPH04194869 A JP H04194869A
- Authority
- JP
- Japan
- Prior art keywords
- viscosity
- toner
- binder resin
- polyolefin
- electrostatic latent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 229920005989 resin Polymers 0.000 claims abstract description 34
- 239000011347 resin Substances 0.000 claims abstract description 34
- 229920000098 polyolefin Polymers 0.000 claims abstract description 29
- 238000004898 kneading Methods 0.000 claims abstract description 28
- 239000003112 inhibitor Substances 0.000 claims abstract description 9
- 229920001577 copolymer Polymers 0.000 claims abstract description 4
- 239000011230 binding agent Substances 0.000 claims description 26
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 101150023883 ethR gene Proteins 0.000 abstract 3
- 239000004743 Polypropylene Substances 0.000 abstract 1
- -1 polypropylene Polymers 0.000 abstract 1
- 229920001155 polypropylene Polymers 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 22
- 239000002245 particle Substances 0.000 description 14
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- 238000013329 compounding Methods 0.000 description 6
- 239000006229 carbon black Substances 0.000 description 4
- 239000003086 colorant Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- YLGXILFCIXHCMC-JHGZEJCSSA-N methyl cellulose Chemical compound COC1C(OC)C(OC)C(COC)O[C@H]1O[C@H]1C(OC)C(OC)C(OC)OC1COC YLGXILFCIXHCMC-JHGZEJCSSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 108091008695 photoreceptors Proteins 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920003066 styrene-(meth)acrylic acid ester copolymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
音束よ■科朋公団
本発明は、圧熱定着される静電潜像現像用トナーの製造
方法に関し、詳しくは、オフセット防止剤としてのポリ
オレフィンが結着樹脂中に均一微細に分散されてなる静
電潜像現像用トナーの製造方法に関する
従米少孜歪
従来、電子写真複写のための静電潜像の現像剤、即ち、
トナーは、一般に、溶融させた熱可塑性樹脂からなる結
着樹脂にカーボンブラック等の着色剤、トナーに所要の
摩擦帯電性を付与するための帯電制御剤粒子、オフセッ
ト防止剤としてのポリオレフィン等の種々の配合剤を混
練、分散させ、冷却した後、ジェットミル等を用いて所
要の粒径にまで微粉砕し、分級することによって、製造
されている。Detailed Description of the Invention The present invention relates to a method for producing a toner for developing an electrostatic latent image that is fixed by pressure and heat. Conventionally, a developer for an electrostatic latent image for electrophotographic copying, namely:
Toner generally includes a binder resin made of a molten thermoplastic resin, a colorant such as carbon black, particles of a charge control agent to give the toner the required triboelectric charging properties, and polyolefin as an anti-offset agent. It is manufactured by kneading and dispersing the ingredients, cooling them, and then pulverizing them to the required particle size using a jet mill or the like and classifying them.
オフセット防止剤は、紙等に転写されたトナー像をヒー
トローラー等によって熱と圧力とを同時に加えて定着さ
せる際に、ヒートローラーへのトナーの移行、付着を防
くために添加される。その機能としては、トナー中に分
散されていたオフセット防止剤が熱と圧力とによってト
ナー表面にしみ出し、ヒートローラーに対して離型性の
ある皮膜をトナー表面に形成することにある。The anti-offset agent is added to prevent the toner from transferring or adhering to the heat roller when the toner image transferred to paper or the like is fixed by simultaneously applying heat and pressure using a heat roller or the like. Its function is that the anti-offset agent dispersed in the toner oozes out onto the toner surface due to heat and pressure, forming a film on the toner surface that is releasable to the heat roller.
このような所謂粉砕法によるトナーが高品質の複写画像
を形成するには、個々のトナー粒子に上記したような配
合剤が均一微細に分散されていることが必要である。配
合剤が個々のトナー粒子に均一微細に分散されていない
ときは、トナーの帯電分布幅が広く、また、配合剤のみ
からなる粒子がトナー粒子に混在し、その結果、複写画
像にかふりを生したり、或いは安定性に欠けたりするほ
か、感光体のフィルミングや機内汚染等が生しる。In order for a toner produced by such a so-called pulverization method to form a high quality copy image, it is necessary that the above-mentioned compounding agents are uniformly and finely dispersed in each toner particle. When the compounding agent is not uniformly and finely dispersed in each toner particle, the charge distribution of the toner is wide, and particles consisting only of the compounding agent are mixed in the toner particles, resulting in fogging of the copied image. In addition to this, there may be problems such as photoreceptor filming and in-machine contamination.
しかし、従来、溶融させた結着樹脂と配合剤とを長時間
、混練しても、尚、結着樹脂中に均一に分散させること
が容易ではなく、配合剤は、個々のトナー粒子に不均一
に分散されることが多い。However, even if the molten binder resin and the compounding agent are kneaded for a long time, it is still not easy to uniformly disperse the compounding agent in the binder resin, and the compounding agent is not mixed into individual toner particles. Often evenly distributed.
紙等に転写されたトナー像が定着過程でヒートローラー
に移行する現象をオフセットと称しているが、この対策
として、結着樹脂に関しては、定着温度（１６０〜２０
０℃程度）での熔融粘度を高くすることと、オフセット
防止剤を添加することとが一般的に行なわれている。オ
フセット防止剤は上記温度ですばやく熔解し、低粘度化
することが望ましく、また、トナー表面にすばやく移行
するためには、結着樹脂との相互作用が小さいことが望
ましい。以上のことから、結着樹脂とオフセット防止剤
とは熔融挙動が全（異なり、また、相互作用が小さいの
で、混練によって均一微細にオフセット防止剤を分散さ
せることは非常に困難である。しかし、オフセット防止
剤の分散が悪ければ、カブリ等の画像欠陥やフィルミン
グ等の問題を生しることがある。The phenomenon in which the toner image transferred to paper etc. is transferred to the heat roller during the fixing process is called offset.As a countermeasure for this, the fixing temperature (160 to 20
It is common practice to increase the melt viscosity at a temperature of about 0° C.) and to add an anti-offset agent. It is desirable that the anti-offset agent melts quickly at the above-mentioned temperature and has a low viscosity, and in order to quickly transfer to the toner surface, it is desirable that its interaction with the binder resin be small. From the above, the melting behavior of the binder resin and the anti-offset agent are completely different, and the interaction is small, so it is very difficult to uniformly and finely disperse the anti-offset agent by kneading.However, If the anti-offset agent is poorly dispersed, problems such as image defects such as fog and filming may occur.
日が２ しようとする課６
本発明者らは、従来の静電潜像現像用トナーの製造にお
ける上記した種々の問題を解決し、特に、オフセット防
止剤としてのポリオレフィンを結着樹脂中に均一微細に
分散させることができる静電潜像現像用トナーの製造方
法を提供することを目的とする。The present inventors solved the various problems described above in the production of conventional toner for developing electrostatic latent images, and in particular, uniformly incorporated polyolefin as an anti-offset agent into a binder resin. An object of the present invention is to provide a method for producing a toner for developing electrostatic latent images that can be finely dispersed.
ｉ を” するための
本発明は、結着樹脂とオフセット防止剤としてのポリオ
レフィンを混練する工程を含む静電潜像現像用トナーの
製造方法において、混練温度における結着樹脂の粘度を
ηえとじ、混練温度における上記ポリオレフィンの粘度
をηＲとするとき、ηＲ／ηア≦５０
なる条件を満足するように、混練温度を設定することを
特徴とする。The present invention provides a method for producing a toner for developing electrostatic latent images, which includes a step of kneading a binder resin and a polyolefin as an offset inhibitor, in which the viscosity of the binder resin at the kneading temperature is The kneading temperature is set so as to satisfy the following condition: ηR/ηa≦50, where ηR is the viscosity of the polyolefin at the kneading temperature.
本発明において、混練温度とは、連続混練機においては
、排出口付近の樹脂温度をいい、ハツチ式混練機におい
ては、混練終了直前の樹脂温度をいう。 。In the present invention, the kneading temperature refers to the resin temperature near the discharge port in a continuous kneader, and refers to the resin temperature immediately before the end of kneading in a hatch type kneader. .
本発明において、結着樹脂は、特に限定されるものでは
ないが、特に、スチレン−（メタ）アクリル酸エステル
共重合体が好ましく用いられる。In the present invention, the binder resin is not particularly limited, but a styrene-(meth)acrylate copolymer is particularly preferably used.
なかでも、１３０℃から１６０ ”Ｃの温度範囲におい
て、５×１０４〜５×１０４ボイズの粘度を有するスチ
レン−（メタ）アクリル酸エステル共重合体が好ましく
用いられる。Among these, a styrene-(meth)acrylic acid ester copolymer having a viscosity of 5 x 104 to 5 x 104 voids in a temperature range of 130°C to 160''C is preferably used.
また、本発明においては、結着樹脂とポリオレフィンと
を混練するに際して、顔料等の帯電制御剤粒子、導電性
粒子、カーボンブラック等の着色剤粒子、磁性粒子等の
種々の特性付与剤が併用されてもよい。このような特性
付与剤は、静電潜像現像用トナーの製造において、既に
よく知られている。Furthermore, in the present invention, when kneading the binder resin and polyolefin, various characteristic imparting agents such as charge control agent particles such as pigments, conductive particles, colorant particles such as carbon black, and magnetic particles are used in combination. It's okay. Such characterization agents are already well known in the production of toners for developing electrostatic latent images.
本発明によれば、必要に応して、上記したような特性付
与剤と共に、オフセット防止剤としてのポリオレフィン
とを混練するに際して、混練温度における結着樹脂の粘
度をη８とし、混練温度における上記ポリオレフィンの
粘度をη２とするとき、
ηＲ／η２≦５０
なる条件を満足するように、混練温度を設定することに
よって、結着樹脂中にオフセット防止剤としてのポリオ
レフィンを均一微細に分散させることができる。According to the present invention, when kneading a polyolefin as an offset inhibitor together with the above-described property imparting agent, the viscosity of the binder resin at the kneading temperature is set to η8, and the polyolefin at the kneading temperature is By setting the kneading temperature so as to satisfy the condition ηR/η2≦50, where η2 is the viscosity of η2, the polyolefin as an offset inhibitor can be uniformly and finely dispersed in the binder resin.
上記ηＲ／ηＲ比（以下、単に粘度比という。）が５０
を越えるときは、ポリオレフィンが溶融し、低粘度であ
って、混練において、結着樹脂とポリオレフィンとがマ
クロに相分離し、結着樹脂中に均一微細に分散しない。The above ηR/ηR ratio (hereinafter simply referred to as viscosity ratio) is 50
When it exceeds the above range, the polyolefin is melted and has a low viscosity, and during kneading, the binder resin and the polyolefin undergo macroscopic phase separation and are not uniformly and finely dispersed in the binder resin.
むしろ、得られるトナーよりもポリオレフィンが大きい
粒子径を有する場合もある。Rather, the polyolefin may have a larger particle size than the resulting toner.
上記粘度比が小さいほど、ポリオレフィンは結着樹脂中
に均一微細に分散するが、しかし、余りに小さいときは
、同時に結着樹脂の粘度がかなり高くなってしまうため
に、ポリオレフィン以外の特性付与剤、例えば、カーボ
ンブラック等の着色剤の結着樹脂中での分散が悪くなっ
たり、混練機の性能上、加工が不可能になったりする。The smaller the above viscosity ratio is, the more uniformly and finely the polyolefin is dispersed in the binder resin. However, if it is too small, the viscosity of the binder resin becomes considerably high, so that property-imparting agents other than polyolefins are used. For example, the dispersion of colorants such as carbon black in the binder resin may become poor, or processing may become impossible due to the performance of the kneader.
このため、本発明においては、上記粘度比は、好ましく
は０．１以上である。即ち、本発明においては、０、１
≦ηＲ／η２ ≦５０
であることが好ましい。Therefore, in the present invention, the viscosity ratio is preferably 0.1 or more. That is, in the present invention, 0, 1
It is preferable that ≦ηR/η2≦50.
通常、オフセット防止剤は、定着過程での高温でのオフ
セット防止のために用いられており、通常の電子写真装
置においては、熱定着ロールの温度ですばやく溶融する
ことが必要である。この熱定着ロールの温度は、通常、
１６０℃以上であるので、本発明においては、オフセッ
ト防止剤であるポリオレフィンは、１６０℃程度で溶融
することが好ましい。かかる融点を有するポリオレフィ
ンとして、本発明においては、特にポサプロピレンが好
ましく用いられる。Generally, offset inhibitors are used to prevent offset at high temperatures during the fixing process, and in ordinary electrophotographic apparatuses, they need to melt quickly at the temperature of the heat fixing roll. The temperature of this heat fixing roll is usually
Since the temperature is 160°C or higher, in the present invention, it is preferable that the polyolefin as an offset inhibitor melts at about 160°C. As a polyolefin having such a melting point, posapropylene is particularly preferably used in the present invention.
光里■四果
以上のように、結着樹脂とオフセット防止剤としてのポ
リオレフィンを混練する工程を含む静電潜像現像用トナ
ーの製造方法において、本発明に従って、混練温度にお
ける結着樹脂の粘度と上記ポリオレフィンの粘度との比
が所定の条件を満足するように、混練温度を設定するこ
とによって、上記ポリオレフィンを結着樹脂中に均一微
細に分散させることができる。As described above, in a method for producing a toner for developing electrostatic latent images that includes a step of kneading a binder resin and a polyolefin as an offset inhibitor, according to the present invention, the viscosity of the binder resin at the kneading temperature and the By setting the kneading temperature so that the ratio to the viscosity of the polyolefin satisfies a predetermined condition, the polyolefin can be uniformly and finely dispersed in the binder resin.
夫隻開
以下に実施例を挙げて本発明を説明するが、本発明はこ
れら実施例により何ら限定されるものではない。EXAMPLES The present invention will be described below with reference to Examples, but the present invention is not limited to these Examples in any way.
粘度の測定とポリオレフィンの分散の評価は以下によっ
た。Measurement of viscosity and evaluation of polyolefin dispersion were carried out as follows.
糀度
レオメトリックス社製のダイナミック・アナライザーを
用い、平行円板状の検出器に結着樹脂の溶融温度以上で
試料を載せ、ＩＨｚ以上の回転数を与えつつ降温して、
粘度と温度との関係を得た。Using a dynamic analyzer manufactured by Koji Rheometrics, a sample was placed on a parallel disc-shaped detector at a temperature above the melting temperature of the binder resin, and the temperature was lowered while applying a rotation speed of IHz or above.
The relationship between viscosity and temperature was obtained.
ポリオレフィンのゝ の評価
混練物をメチルエチルケトンに加え、結着樹脂を溶解さ
せ、スライドガラスに採取し、光学顕微鏡で観察した。Evaluation of Polyolefin The kneaded product was added to methyl ethyl ketone to dissolve the binder resin, sampled on a slide glass, and observed under an optical microscope.
ポリオレフィンはメチルエチルケトンに溶解しないので
、上記によって、ポリオレフィンの粒度や形状を観察し
た。Since polyolefin does not dissolve in methyl ethyl ketone, the particle size and shape of polyolefin were observed as described above.
実施例１及び比較例１．２
スチレン−メタクリル酸ブチル共重合体（重量平均分子
量２Ｘ１０５、数平均分子量５．５×１０４）１００重
量部、［スビロンブラックＴＲＨＪ ２重量部、カーボ
ンブラック（日本イージー社製ケッチエンブラックＥＣ
）３重量部及びポリオレフィンワックス（三洋化成工業
■製ビスコール５５０Ｐ）３重量部を混合し、ラボ・プ
ラストミル（東洋精機製作断裂）にて混練した。混練後
のポリオレフィンの分散を評価した。Example 1 and Comparative Example 1.2 100 parts by weight of styrene-butyl methacrylate copolymer (weight average molecular weight 2 x 105, number average molecular weight 5.5 x 104), 2 parts by weight of Subiron Black TRHJ, carbon black (Japan Easy Manufactured by Ketchen Black EC
) and 3 parts by weight of polyolefin wax (Viscol 550P manufactured by Sanyo Chemical Industries, Ltd.) were mixed and kneaded in a Labo Plastomill (manufactured by Toyo Seiki). The dispersion of the polyolefin after kneading was evaluated.
実施例２及び比較例３．４
上記混合物を二軸押出機にて溶融混練した。得られた混
練物を冷却し、ジェット粉砕機にて粉砕し、次いで、風
力分級機を用いて、粒子径約５〜２０μｍの粒子を得た
。Example 2 and Comparative Example 3.4 The above mixtures were melt-kneaded in a twin-screw extruder. The obtained kneaded product was cooled and pulverized using a jet pulverizer, and then using an air classifier to obtain particles having a particle size of about 5 to 20 μm.
次に、このマスターバッチ１００重量部とケイ酸微粉０
．３重量部（日本アエロジル社製Ｒ−９７２）とを乾式
混合し、トナーを得た。Next, 100 parts by weight of this masterbatch and 0 parts of silicic acid fine powder were added.
．． 3 parts by weight (R-972 manufactured by Nippon Aerosil Co., Ltd.) were dry mixed to obtain a toner.
このトナーをトナー濃度６重量％となるようにキャリア
（日本鉄粉社製ＥＦＶ２５０）と混合し、二成分系トナ
ーを調製した。このトナーを市販普通紙静電複写機（三
洋電機■製ＳＦＴ−１１０２ＡＺ）に適用し、１０００
０枚の連続複写を行なって、画像評価をした結果を第１
表に示す。This toner was mixed with a carrier (EFV250 manufactured by Nippon Tetsuko Co., Ltd.) so that the toner concentration was 6% by weight to prepare a two-component toner. This toner was applied to a commercially available plain paper electrostatic copying machine (SFT-1102AZ manufactured by Sanyo Electric Co., Ltd.) and
The results of image evaluation after continuous copying of 0 sheets are
Shown in the table.
特許出願人 ハンド−化学株式会社 代理人 弁理士 牧 野 逸 部Patent applicant: Hand Chemical Co., Ltd. Agent Patent Attorney Itsu Makino
Claims (4)
ィンを混練する工程を含む静電潜像現像用トナーの製造
方法において、混練温度における結着樹脂の粘度をη＿
Ｒとし、混練温度における上記ポリオレフィンの粘度を
η＿Ｐとするとき、η＾Ｒ／η＿Ｐ≦５０ なる条件を満足するように、混練温度を設定することを
特徴とする静電潜像現像用トナーの製造方法。(1) In a method for producing a toner for developing an electrostatic latent image that includes a step of kneading a binder resin and a polyolefin as an offset inhibitor, the viscosity of the binder resin at the kneading temperature is η_
Production of a toner for developing electrostatic latent images, characterized in that the kneading temperature is set so as to satisfy the following condition: η^R/η_P≦50, where R is the viscosity of the polyolefin at the kneading temperature and η_P. Method.
有し、且つ、この温度範囲において、５×１０＾３〜５
×１０＾４ポイズの粘度を有することを特徴とする請求
項第１項記載の静電潜像現像用トナーの製造方法。(2) The binder resin has a melting point in the range of 130°C to 160°C, and in this temperature range, 5 × 10^3 to 5
2. The method for producing an electrostatic latent image developing toner according to claim 1, wherein the toner has a viscosity of x10^4 poise.
ル共重合体であることを特徴とする請求項第２項記載の
静電潜像現像用トナーの製造方法。(3) The method for producing a toner for developing electrostatic latent images according to claim 2, wherein the binder resin is a styrene-(meth)acrylate copolymer.
徴とする請求項第１項記載の静電潜像現像用トナーの製
造方法。(4) The method for producing a toner for developing electrostatic latent images according to claim 1, wherein the polyolefin is posapropylene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2320203A JPH04194869A (en) | 1990-11-22 | 1990-11-22 | Manufacture of electrostatic latent image developing toner |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2320203A JPH04194869A (en) | 1990-11-22 | 1990-11-22 | Manufacture of electrostatic latent image developing toner |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04194869A true JPH04194869A (en) | 1992-07-14 |
Family
ID=18118861
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2320203A Pending JPH04194869A (en) | 1990-11-22 | 1990-11-22 | Manufacture of electrostatic latent image developing toner |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04194869A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1372043A2 (en) * | 2002-06-13 | 2003-12-17 | Heidelberger Druckmaschinen Aktiengesellschaft | Electrophotographic toner with uniformly dispersed wax |
-
1990
- 1990-11-22 JP JP2320203A patent/JPH04194869A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1372043A2 (en) * | 2002-06-13 | 2003-12-17 | Heidelberger Druckmaschinen Aktiengesellschaft | Electrophotographic toner with uniformly dispersed wax |
| JP2004163879A (en) * | 2002-06-13 | 2004-06-10 | Heidelberger Druckmas Ag | Electrophotographic toner in which wax is uniformly dispersed |
| EP1372043A3 (en) * | 2002-06-13 | 2004-12-29 | Eastman Kodak Company | Electrophotographic toner with uniformly dispersed wax |
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